高效液相色谱法测定化妆品中5种水杨酸酯紫外吸收剂  

Determination of 5 salicylic acid ester ultraviolet absorbers in cosmetics by high performance liquid chromatography

作　　者：刘小娟[1] 陈桂琴 黄佳颖 梁柱业 肖树雄[1] LIU Xiaojuan;CHEN Guiqin;HUANG Jiaying;LIANG Zhuye;XIAO Shuxiong(Guangdong Institute for Drug Control,NMPA Key Laboratory for Safety Risk Assessment of Cosmetics,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所国家药品监督管理局化妆品风险评估重点实验室,广州510663

出　　处：《化学分析计量》2023年第11期31-35,共5页Chemical Analysis And Meterage

基　　金：广东省医学科学技术研究基金面上项目(B2021160)。

摘　　要：建立了高效液相色谱法测定化妆品中5种水杨酸酯紫外吸收剂的检测方法。样品经四氢呋喃-甲醇-0.1%(体积分数)甲酸溶液混合溶液(体积比为60∶30∶10)超声提取,使用CAPCELL PAK MGⅡC18色谱柱(250 mm×4.6mm,5μm)分离,柱温为30℃,流动相为四氢呋喃-甲醇-0.1%甲酸溶液,流量为1.0 mL/min,进样体积为10μL,检测波长为305 nm,梯度洗脱分析。乙二醇单水杨酸酯、水杨酸苯酯、水杨酸苄酯、水杨酸己酯、丁基辛醇水杨酸酯5种水杨酸酯紫外吸收剂在质量浓度为10~200μg/mL范围内与色谱峰面积具有良好的线性关系,相关系数不小于0.999 5,检出限为2 ng,定量限为6 ng,平均回收率为93.7%~105.1%,相对标准偏差为1.1%~4.5%(n=6),对照品溶液在2个月内量值稳定。该方法操作简便、灵敏度高,可用于化妆品中紫外吸收剂的检测。A high-performance liquid chromatography method was established for the determination of five salicylic acid ester ultraviolet absorbers in cosmetics.The sample was ultrasonically extracted by a mixture of tetrahydrofuran,methanol and 0.1%(volume fraction) formic acid solution(60/30/10) by using CAPCELL PAK MGⅡC18 chromatography column(250 mm×4.6 mm,5 μm).The column temperature was 30 ℃,the mobile phase was tetrahydrofuran-methanol-0.1% formic acid solution with the flow rate of 1.0 mL/min,and the injection volume was 10 μL.The detection wavelength was 305 nm,and gradient elution analysis was performed.The mass concentrations of five salicylic such as 2-hydroxyethyl salicylate,phenyl salicylate,benzyl salicylate,hexyl salicylate and butyl octanol salicylate were between 10-200 μg/mL.There was a good linear relationship between the mass concentration of the aids compounds and the chromatographic peak area with the correlation coefficients not less than 0.999 5,the detection limits were all 2 ng,the quantification limits were all 6 ng,and the average recovery rate was 93.7%-105.1% with the relative standard deviation of 1.1%-4.5%(n=6).The reference solution had stable value in 2 months.This method is easy to operate and highly sensitive,and it can be used for the detection of ultraviolet absorbents in cosmetics.

关 键 词：高效液相色谱法 乙二醇单水杨酸酯 水杨酸苯酯 水杨酸苄酯 水杨酸己酯 丁基辛醇水杨酸酯 紫外吸收剂 

分 类 号：O657.7[理学—分析化学]